Download - Nist Dtsa-II Guide

7/18/2019 Nist Dtsa-II Guide

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NIST DTSA-II ( Son of DTSA ):

Step-by-Step

Dale E. Newbury (grateful user)National Institute of Standards and Technology

Gaithersburg, MD 20899-8370


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NIST-NIH Desktop Spectrum Analyzer (DTSA)


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Photon Energy (keV)

Log

Intensity

FeK

FeK

CaK

CaK

SiK AlK

FeL

OK

CaL

NIST Glass K411

E0= 20keV

Inside specimen

After specimen absorption

After EDS window absorption

After EDS broadening (145 eV)

Spectral Simulation with DTSA

For 16 years, I have heard: When will you have DTSA for the pc?


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NIST DTSA-II

Created by Nicholas Ritchie of NIST ([email protected]),

inspired by NIST-NIH Desktop Spectrum Analyzer (DTSA) invented

1990-92 by Chuck Fiori (NIH and NIST) and Carol Swyt-Thomas (NIH),

and then further developed by Carol and Bob Myklebust (NIST).


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NIST DTSA-II





DTSA ran only on Macintosh, and then only up to system 10. (New

Macs wont run DTSA) A painful question heard many, many times:

When wil l you have DTSA for the pc? DTSA-II is the long awaited

answer!!


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NIST DTSA-II








answer!!

DTSA-II is written in Java and operates on Mac, pc, UNIX, Linux.


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NIST DTSA-II








answer!!


DTSA-II is NOTDTSA! Nicholas started from scratch and used DTSA

as a guide to develop DTSA-II.


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NIST DTSA-II








answer!!




DTSA-II is being continually improved and the latest version can be

downloaded for free athttp://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html


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NIST DTSA-II








answer.




DTSA-II is being continually improved and the latest version can be

downloaded for free athttp://www.cstl.nist.gov/div837/837.02/epq/dtsa2/index.html

Tools currently embedded in DTSA-II:


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Basic operations

Opening and manipulating spectral files


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Display and overlay spectra with various scaling options on linear/log/sqrt axes

Basic DTSA-II display window


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Spectrum f ile selection window


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A single spectrum is selected.

Spectrum preview opens in this window.


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Display and overlay spectra with various scaling options on linear/log/sqrt axes

OK or double click loads spectrum

Basic display of single spectrum

Intensity (x-ray counts)

Energy scale in eV

Opened

spectra are

listed hereSpectrum information

from header


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But wait!

A brilliant feature, the Report is going to

record your actions. A daily diary of actions

(file named by date) is automatically saved.


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But wait! A brilliant feature, the Report is going to record your actions. A

daily diary of actions (file named by date) is automatically saved.

The Report is a great

feature for those of us

approaching geezerhood.

Now, what was I saying?


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Open several spectra at a time:

Holding down SHIFT key gives a continuous run

Preview of spectra in this window


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To open several spectra at a time:Holding down CTRL key allows multiple separate

selections


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3 spectrum files have opened

Note data from header

List of loadedspectra.

Highlighted

are displayed

When spectra have

differences in the

header data, only

the terms in common

will be displayed

when more than one

spectrum is selected


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Basic operations


Display of spectra


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Changing the vertical axis scale:

Method 1: Use arrows: x2 or x5 /2 or /5

This arrow button restores full spectrum display

Method 2: Mouse in y-axis number field; click and drag up or down



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Changing the vertical axis scale:

Method 3

Right click in spectrum display brings up this

Window; choose zoom in or zoom out; this

operation can be repeated.

Note: Zoom to all restores full spectrum


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Changing the vertical axis

scale from linear to log

1. Right click in spectrum

window.

2. Select Ordinate scale

3. Select Log


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scale from linear to log

1. Right click in spectrum window.


3. Select Log


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scale from linear to square root

1. Right click in spectrum window.


3. Select Square root


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Changing the horizontal axis scale: Method 1

1. Click a preset to show 0-5, 010, 0-15, or 0-20 keV


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Click a preset to show 0-5, 010, 0-15, or 0-20 keV

0 5 keV is shown


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Changing the horizontal axis scale: method 2

Right click in spectrum field

Choose create an ROI


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1. Right click in spectrum field

2. Choose create an ROI

3. Define start and end energies


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1. Right click in spectrum field

2. Choose create an ROI

3. Define start and end energies

4. OK This action creates yellow ROI

5. Click this icon to fully expand this ROIor

6. Click within ROI and select

Zoom to region

B i di l f i l t


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6. Final display of 3.0 5.0 keV range



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1. Double click and sweep an ROI

(low to high energy) creating yellow ROI

2. Immediate display of ROI parameters



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3. Click icon to expand

OR

4. Right click within yellow ROI

5. Select zoom to region



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3. Click icon to expand

OR

4. Right click within yellow ROI

5. Select zoom to region

6. Final display of expanded ROI


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Basic operations


Display of spectra

Peak labeling (manual only)

Peak Labeling


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KLM selection

One spectrum

selected from list.

Peak Labeling

Peak Labeling


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To make labels stick

click these check boxes

Peak Labeling

Peak Labeling


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Labeled Spectrum

Peak Labeling

Peak Labeling


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Choosing the

peak label style

Peak Labeling

Peak Labeling


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Choosing the

peak label style

IUPAC Long labels

Peak Labeling

Peak Labeling


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Choosing the

peak label style

Siegbahn labels

Peak Labeling


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Basic operations


Peak labeling (manual only)

Exporting spectra for publication (Gnuplot)

Export ing spectrum for publication as gnuplot


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Export ing spectrum for publication as gnuplot


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Publication-quality graphics from Gnuplot

Comparing spectra from different EDS spectrometers,


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p g p p

or from different dates from the same EDS:

The issue of EDS calibration A spectrum is recorded with calibration data: eV/channel, zero offset,

number of channels (depending on manufacturer, this data may or

may not be embedded in the .msa header).

When a spectrum is read into DTSA-II, the calibration information ischecked against the current calibration. If there is a mismatch, a

message prompts the analyst.

Spectrum Calibration


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When attempting to open

a spectrum file with

a different calibration,this message appears:

Th i f EDS lib ti


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The issue of EDS calibration A spectrum is recorded with calibration data: eV/channel, zero offset,

number of channels (depending on manufacturer, this data may or

may not be embedded in the .msa header).

When a spectrum is read into DTSA-II, the calibration information is

checked against the current calibration. If there is a mismatch, a

message prompts the analyst.

The analyst then has two choices:

1. Change the detector selection to match the incoming spectrum

2. Accept the incoming spectrum but display it according to the current

calibration information. (Note: the incoming spectrum will retain its

calibration data so that when it is the only spectrum being displayed, its

own calibration will be applied.)


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Comparing multiple spectra Matching to a particular ROI

Comparing multiple spectra


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We wish to match the spectra for the

integral of SiK,

Step 1: Click and swipe across SiK,

peak to define ROI for matching.



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We wish to match the spectra

for the integral of SiK,

Step 2: Right click and select

Spectrum Comparison,

then Region integral



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Result shows Si peaks matched

Spectrum sub sampling tool


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Spectrum sub-sampling tool

Take an experimentally measured spectrum and create

one or more sub-samples, that is, equivalent spectra

that would have been collected at lower dose.

Sub-sampled spectra are useful for statistical studies.

e.g., how does detection limit vary with dose.

Spectrum sub-sampling : creating equivalent spectra for other doses


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Starting

measured spectrum



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Equivalent dose factor;

set to 5% for this calculation

Number of synthesized

spectra, each with

different statistics

Random

Number

seed



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3 sub-sampled

spectra added to l ist

Note: for this example,

5% dose lowered the

intensity scale by a

factor of 20, as expected



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Each sub-sampled

spectrum is prepared

with different random

statistics.


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Background fitting tool

Background Fitting


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Background Fitting


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Enter material

composition

Background Fitting


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Enter material

composition

Background Fitting


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Fit with automatic

placement of

background ROIs

Background Fitting


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Fit with maual

placement of

background ROIs

Background Fitting


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Comparison of

manualand automatic

placement of

background ROIs

DTSA-II Simulation Mode


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EDS spectra calculated from

1. First principles, using best available cross sections

and physical data (flat, bulk target only)

Simulation Alien


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Simulation Alien: selecting Analytical Simulation


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Simulation Alien: specifying composit ion


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Simulation Alien: target composition


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Simulation Alien: instrument configuration


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Simulation Alien: Other opt ions not invoked


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Simulation Alien


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Hit Finish when Progress

bar is fi lled

Simulation Alien


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Physics result

Simulation Al ien: Other options invoked


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Counting statistics appropriate to

the dose and spectrometer effic iency

are applied for the specified number of

replicates.

Simulation Alien


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the dose and spectrometer efficiency

are applied to the physics result for the

specified number of replicates.

Simulation Alien


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the dose and spectrometer efficiency

are applied to the physics result for the

specified number of replicates.

Comparison of

Physics Resultand

after applying

counting statistics



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2. Monte Carlo electron trajectory simulation forvarious specimen configurations:

1. Flat, bulk

2. Layer on bulk 3. Inclusion (hemisphere) embedded in bulk

4. Spherical particle on substrate

5. Cubic particle on substrate

Simulation Alien: Monte Carlo simulation of a 1 m K411 glass sphere on a C substrate


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Invoke x-ray

generation

images



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Report tab:

Generated and

emitted intensities



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X-ray

production

images

under

Reporttab.



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X-ray

production

images

under

Reporttab.Trajectory View

Simulation Alien: Monte Carlo simulation trajectories can be viewed with Cosmo Player


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View along X-axis (rotated view from Y-axis)



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View along Y-axis

View along the beam


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1 m

View along the beam


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View from bottom of particle


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2. Monte Carlo electron trajectory simulation forvarious specimen configurations:

1. Flat, bulk

2. Layer on bulk 3. Inclusion (hemisphere) embedded in bulk

4. Spherical particle on substrate

5. Cubic particle on substrate

Simulation Alien: Monte Carlo simulation of a 1 m SiO2 hemisphere in FeS2


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E0= 20 keV

1-m inclusion of SiO2in FeS2



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E0= 20 keV

1-m inclusion of SiO2in FeS2



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DTSA-II: Quantitative Analysis


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ZAF analysis against standards

Standards are used to extract neededpeak references for MLLS fit.

Report contains pertinent data (ZAF

factors, weight%, atom%, normalizedweight%; 1statistics)


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Select File


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Choose a spectrum fi le


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Continue

specifying

needed

spectra


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Access

Finder

to select

spectra


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Report contains

ZAF details


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Residuals after fitt ing peaks

Note: symmetric structure of residuals

at peak positions implies that thepeak references used are

appropriate for this unknown.

Comparison of

M d d


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Measuredand

Simulated FeS spectra

Note good fit for

FeK and S K, but poorfit for FeL

Comparison of

Measured and


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Measuredand


Comparison ofMeasuredand


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after region integral

scaling

Adding a new detector to the list under Preferences


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